Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran

A facile procedure for extracting and determining seven neonicotinoids was developed. Water was the only extraction solvent without phase separation and cleanup steps. The method was validated according to European Union standards, and the values obtained were compared with the criteria. The accurac...

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Main Authors: Osama I. Abdallah, Rania M. Abd El-Hamid, Nevein S. Ahmed, Saleh S. Alhewairini, Sherif B. Abdel Ghani
Format: Article
Language:English
Published: MDPI AG 2024-04-01
Series:Foods
Subjects:
Online Access:https://www.mdpi.com/2304-8158/13/7/1106
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author Osama I. Abdallah
Rania M. Abd El-Hamid
Nevein S. Ahmed
Saleh S. Alhewairini
Sherif B. Abdel Ghani
author_facet Osama I. Abdallah
Rania M. Abd El-Hamid
Nevein S. Ahmed
Saleh S. Alhewairini
Sherif B. Abdel Ghani
author_sort Osama I. Abdallah
collection DOAJ
description A facile procedure for extracting and determining seven neonicotinoids was developed. Water was the only extraction solvent without phase separation and cleanup steps. The method was validated according to European Union standards, and the values obtained were compared with the criteria. The accuracy values were between 99.8% (thiamethoxam) and 106.8% (clothianidin) at the spiking levels of 0.01, 0.1, and 1 mg/kg in the tested matrices. The precision as pooled RSD values was ≤6.1% (intra-day) and ≤6.9% (inter-day). The limit of quantification was set and tested at 0.01 mg/kg. The matrix effect was evaluated, and all matrices had a suppressive effect. The matrix of the cucumber was the most effective, with −20.9% for dinotefuran and an average of −9.8% for all compounds, while the tomato matrix had the slightest effect. Real marketed samples were analyzed using the developed and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methods; the results were not significantly different. A supervised field trial was conducted in the open field to study the dissipation patterns of imidacloprid and dinotefuran in tomatoes. The dissipation of both compounds followed first-order kinetics. The half-life (T<sub>½</sub>) values were 3.4 and 2.5 days, with dissipation rates k of 0.2013 and 0.2781 days, respectively. Following the EU-MRL database, the calculated pre-harvest interval (PHI) values were 7 and 14 days for imidacloprid and dinotefuran, respectively, and 3 days for both compounds following Codex Alimentarius regulations. The risk of imidacloprid and dinotefuran residues was estimated from chronic and acute perspectives. The risk factors of dinotefuran were lower than those of imidacloprid. Nonetheless, the highest expected residues of both compounds were below the tolerance limits.
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spelling doaj.art-500d8b1731214a5694f4c848e34fe9e22024-04-12T13:18:41ZengMDPI AGFoods2304-81582024-04-01137110610.3390/foods13071106Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and DinotefuranOsama I. Abdallah0Rania M. Abd El-Hamid1Nevein S. Ahmed2Saleh S. Alhewairini3Sherif B. Abdel Ghani4Department of Pesticide Residues and Environmental Pollution, Central Agricultural Pesticide Laboratory, Agricultural Research Center, Giza 12618, EgyptDepartment of Pesticide Residues and Environmental Pollution, Central Agricultural Pesticide Laboratory, Agricultural Research Center, Giza 12618, EgyptDepartment of Pesticide Residues and Environmental Pollution, Central Agricultural Pesticide Laboratory, Agricultural Research Center, Giza 12618, EgyptDepartment of Plant Protection, College of Agriculture and Food, Qassim University, P.O. Box 6622, Buraydah 51452, Saudi ArabiaDepartment of Plant Protection, College of Agriculture and Food, Qassim University, P.O. Box 6622, Buraydah 51452, Saudi ArabiaA facile procedure for extracting and determining seven neonicotinoids was developed. Water was the only extraction solvent without phase separation and cleanup steps. The method was validated according to European Union standards, and the values obtained were compared with the criteria. The accuracy values were between 99.8% (thiamethoxam) and 106.8% (clothianidin) at the spiking levels of 0.01, 0.1, and 1 mg/kg in the tested matrices. The precision as pooled RSD values was ≤6.1% (intra-day) and ≤6.9% (inter-day). The limit of quantification was set and tested at 0.01 mg/kg. The matrix effect was evaluated, and all matrices had a suppressive effect. The matrix of the cucumber was the most effective, with −20.9% for dinotefuran and an average of −9.8% for all compounds, while the tomato matrix had the slightest effect. Real marketed samples were analyzed using the developed and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methods; the results were not significantly different. A supervised field trial was conducted in the open field to study the dissipation patterns of imidacloprid and dinotefuran in tomatoes. The dissipation of both compounds followed first-order kinetics. The half-life (T<sub>½</sub>) values were 3.4 and 2.5 days, with dissipation rates k of 0.2013 and 0.2781 days, respectively. Following the EU-MRL database, the calculated pre-harvest interval (PHI) values were 7 and 14 days for imidacloprid and dinotefuran, respectively, and 3 days for both compounds following Codex Alimentarius regulations. The risk of imidacloprid and dinotefuran residues was estimated from chronic and acute perspectives. The risk factors of dinotefuran were lower than those of imidacloprid. Nonetheless, the highest expected residues of both compounds were below the tolerance limits.https://www.mdpi.com/2304-8158/13/7/1106green solventneonicotinoid pesticidesresidue dissipationmethod validationrisk assessment
spellingShingle Osama I. Abdallah
Rania M. Abd El-Hamid
Nevein S. Ahmed
Saleh S. Alhewairini
Sherif B. Abdel Ghani
Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran
Foods
green solvent
neonicotinoid pesticides
residue dissipation
method validation
risk assessment
title Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran
title_full Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran
title_fullStr Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran
title_full_unstemmed Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran
title_short Development of Green and Facile Sample Preparation Method for Determination of Seven Neonicotinoids in Fresh Vegetables, and Dissipation and Risk Assessment of Imidacloprid and Dinotefuran
title_sort development of green and facile sample preparation method for determination of seven neonicotinoids in fresh vegetables and dissipation and risk assessment of imidacloprid and dinotefuran
topic green solvent
neonicotinoid pesticides
residue dissipation
method validation
risk assessment
url https://www.mdpi.com/2304-8158/13/7/1106
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